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超高效液相色谱-串联质谱法同时检测人血浆中11种镇静催眠药浓度∗

安静 董占军 魏欣 白万军 宋浩静

医药导报2016,Vol.35Issue(9):938-942,5.
医药导报2016,Vol.35Issue(9):938-942,5.DOI:10.3870/j.issn.1004-0781.2016.09.007

超高效液相色谱-串联质谱法同时检测人血浆中11种镇静催眠药浓度∗

Detection and Validated Quantification of 11 Sedative-Hypnotics in Human Plasma by UPLC-MS/MS Method

安静 1董占军 1魏欣 1白万军 1宋浩静1

作者信息

  • 1. 河北省人民医院药学部,石家庄 050051
  • 折叠

摘要

Abstract

Objective To develop a rapid ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/ MS) for determination of 11 sedative-hypnotics in human plasma. Methods The plasma samples were extracted with dichloromethane:n-hexane:acetoacetate (5∶4∶1). The separation was performed on a Waters ACQUITY UPLC HSS T3 column (2.1 mm×100 mm,1.8 μm) using the mobile phase composed of acetonitrile-0.1% ammonium solution at a flow rate of 0.2 mL•min-1 in gradient elution mode. The detection was performed on a triple quadrupole tandem mass spectrometer by multiple reaction monitoring (MRM) via electrospray ionization (ESI) source in positive mode. Results Good linear relation was obtained over the investigated concentration range, with all correlation coefficients higher than 0.99. The limit of detection was 200 pg•mL-1 for dexzopiclone,and 10- 20 pg•mL-1 for other sedative-hypnotics. The intra- and inter-day RSD of 11 sedative-hypnotics were no more than 15.0%. The recoveries were in the range of 72.3%-108.0%, and the matrix effects were approximately 0.86- 1. 12. Conclusion The method is rapid, sensitive and reliable, and suitable for the simultaneous determination of 11 sedative-hypnotics in human plasma.

关键词

镇静催眠药/色谱,超高效液相/质谱,串联/血药浓度

Key words

Sedative-Hypnotics/Chromatography, ultra high performance liquid/Mass spectromety, tandem/Human plasma concentration

分类

医药卫生

引用本文复制引用

安静,董占军,魏欣,白万军,宋浩静..超高效液相色谱-串联质谱法同时检测人血浆中11种镇静催眠药浓度∗[J].医药导报,2016,35(9):938-942,5.

基金项目

河北省科技计划项目(14273002D) (14273002D)

医药导报

OACSTPCD

1004-0781

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